50 results about "Meta-Chloroperoxybenzoic acid" patented technology

The invention relates to the technical field of fabric preparation, in particular to environment-friendly breathable polyester silk fabric and a preparation process thereof. The preparation method comprises the following steps: preparing an epoxy polyurethane emulsion by taking glycidyl as an end-capping reagent; eugenol and phenyl dichlorophosphate are used as raw materials to react, and m-chloroperoxybenzoic acid is used as an oxidizing agent to prepare an epoxy flame retardant; the preparation method comprises the following steps: carrying out reaction on N, N-diethylaminopropyl methyl dimethoxy silane and epoxy chloropropane to obtain epoxy organosilicon quaternary ammonium salt; mixing the epoxy-based polyurethane emulsion, the epoxy-based flame retardant, the epoxy-based organosilicon quaternary ammonium salt and the curing agent, and modifying the polyester silk; preparing bio-based spinning fibers from a mixed solution of a carboxymethyl cellulose solution and a chitosan solution through an electrostatic spinning technology, and then blending the bio-based spinning fibers with the modified polyester to obtain the polyester fabric. The polyester silk fabric prepared by the method has good flame retardant property, antibacterial property and air permeability, and part of materials are renewable materials, so that the polyester silk fabric is economical and environment-friendly and meets the requirement of green development.

The invention discloses phenolic anti-aging styrene-butadiene rubber and a preparation method thereof, and relates to the technical field of rubber functional modification.The preparation method of the phenolic anti-aging styrene-butadiene rubber comprises the steps that firstly, epoxidation reaction is conducted on styrene-butadiene rubber through metachloroperbenzoic acid, then epoxy group ring-opening reaction is conducted on the styrene-butadiene rubber and hydrochloric acid, and the phenolic anti-aging styrene-butadiene rubber is obtained. And finally, carrying out esterification reaction with a phenolic anti-aging agent to prepare the phenolic anti-aging styrene-butadiene rubber. According to the invention, a phenol-containing anti-aging functional side chain is grafted in a styrene-butadiene rubber molecular chain through an epoxy-ring opening-esterification three-step reaction, so that the thermal oxidation resistance and ozone aging resistance of the styrene-butadiene rubber are improved, and meanwhile, the problem that a micromolecular anti-aging agent is easy to migrate in a rubber matrix due to relatively poor compatibility is solved.

The invention discloses an acid-alkali-resistant high-weather-resistant insulating powder coating as well as a preparation method and application thereof in the aspect of sound screens of high-speed guardrails, and relates to the technical field of fluorocarbon resin powder coatings. The insulating powder coating with acid and alkali resistance and high weather resistance is prepared from the following raw materials in parts by weight: 15 to 25 parts of fluorocarbon resin, 40 to 50 parts of polyester resin, 5 to 12 parts of curing agent, 0.5 to 2 parts of accelerant, 3 to 8 parts of corrosion-resistant agent, 2 to 5 parts of weather-resistant agent, 1 to 2 parts of flatting agent, 0.3 to 1 part of benzoin and 10 to 15 parts of inorganic nano filler. The preparation method comprises the following steps: reacting 4-trifluoromethylphenol with 6-bromo-1-hexene to obtain an intermediate 1, generating an intermediate 2 from the intermediate 1 under the action of m-chloroperoxybenzoic acid, and reacting the intermediate 2 with amino-terminated polyether to generate the corrosion-resistant agent. The acid-base-resistant high-weather-resistant insulating powder coating prepared by the invention has good acid-base resistance, heat aging resistance and light aging resistance.

The invention discloses a semi-solid lithium battery separator and a semi-solid lithium battery, and relates to the technical field of battery materials. When preparing the semi-solid lithium battery separator, the present invention oxidizes octavinyl octasilsesquioxane with meta-chloroperbenzoic acid to obtain epoxidized POSS; reacts epoxidized POSS with N,N-dimethylallylamine and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in sequence to obtain functionalized POSS; cellulose is oxidized with sodium periodate to obtain oxidized cellulose; oxidized cellulose is reacted with melamine to obtain modified cellulose; 4,4'-diaminodiphenyl ether is polycondensed with 3,3',4,4'-biphenyltetracarboxylic dianhydride to obtain a polyamic acid solution; polyamic acid solution, polyvinyl pyrrolidone, functionalized POSS, and modified cellulose are uniformly mixed, coated and cured to obtain a semi-solid lithium battery separator. The semi-solid lithium battery separator prepared by the present invention has excellent flame retardancy, ionic conductivity, high thermal stability and mechanical properties.

The invention discloses a phototherapy reagent and a preparation method and application thereof. The preparation method comprises the following steps: 1-[4-(diethylamino) phenyl]-ethane-1-ketone and 4-methoxybenzaldehyde are subjected to a condensation reaction in a NaOH ethanol solution, and a product and nitromethane are subjected to addition; performing condensation and addition on the other groups of raw materials by the same method; cyclizing the two addition products with ammonium acetate, and coordinating with boron trifluoride diethyl etherate to obtain NHM; carrying out substitution reaction on the NHM and sodium nitrite to obtain NOO; and oxidizing NOO by m-chloroperoxybenzoic acid to obtain NNOO. The reagent can target a tumor hypoxia microenvironment, hypoxia monitoring is achieved, NO is released through photostimulation for tumor gas therapy, meanwhile, the secondary amplification photo-thermal therapy effect is achieved, preparation is controllable, diagnosis and treatment are integrated, and the reagent is sensitive, safe and suitable for biomedical research and clinical diagnosis.

The application relates to the technical field of chemical synthesis, in particular to a synthesis method of a key intermediate of pentconazole, which comprises the following steps: S1, Witting-Horner reaction of 2,4-dichlorobenzophenone and (diethoxy) phosphoethyl acetate under the action of a strong base to generate 3-(2,4-dichlorophenyl)-2-en-hexanoic acid ethyl ester; S2, Prilezhaev epoxidation reaction of 3-(2,4-dichlorophenyl)-2-en-hexanoic acid ethyl ester and meta-chloro peroxybenzoic acid to generate 3-(2,4-dichlorophenyl)-2,3-epoxy-hexanoic acid ethyl ester; and S3, base hydrolysis and acidification of 3-(2,4-dichlorophenyl)-2,3-epoxy-hexanoic acid ethyl ester to obtain a key intermediate 2-(2,4-dichlorophenyl) pentanal of pentconazole. The application has the effects of higher reaction yield, lower toxicity of reaction raw materials and more gentle reaction conditions.

The present invention discloses a process for preparing m-chloroperbenzoic acid by using a molecular sieve catalyst, belonging to the technical field of chemical catalytic preparation, and comprising the following steps: S1, dissolving m-chlorobenzoic acid in an organic solvent, adding the molecular sieve catalyst, uniformly stirring, and then dropwise adding an aqueous oxidant solution with a mass fraction of 15% to 30% for an oxidation reaction; S2, after the oxidation reaction is completed, separating the molecular sieve by using a filter for the next reaction; S3, after separation, extracting and separating the organic phase, distilling and recovering the organic solvent to obtain m-chloroperbenzoic acid crystals. The present invention overcomes the defects and deficiencies in the existing process methods, such as low effective yield and serious wastewater pollution. A solid molecular sieve is used as the catalyst. The catalyst has stable properties, simple separation, the solvent can be recycled and reused in the process, the product yield is high, environmental problems caused by other oxidation methods are avoided, and it is beneficial to large-scale industrial production.

This invention belongs to the field of pharmaceutical technology, specifically providing a new method for synthesizing crude dotenoradine. This invention uses 2-aminobenzylthiol as the starting material, and obtains crude dotenoradine through cyclization reaction, first oxidation reaction, acylation reaction, and second oxidation reaction. It mainly utilizes the relatively weak oxidizing property of hydrogen peroxide, which makes it difficult to directly oxidize sulfide (1) to sulfone (2') in a high yield. Instead, relatively expensive m-chloroperoxybenzoic acid is still needed to complete the oxidation. This invention controls the oxidation of sulfide by controlling the amount of hydrogen peroxide and the composite catalyst and catalytic aid, so that most of the oxidation products remain in the sulfoxide structure (2) and are difficult to completely convert to the sulfone structure. After another oxidation reaction, the amount of m-chloroperoxybenzoic acid can be reduced relatively much, thus reducing the synthesis cost of crude dotenoradine.

The application provides a preparation method of dydrogesterone, which comprises the following steps: performing a selective epoxidation reaction on a compound I in a first solution containing meta-chloroperoxybenzoic acid and hydrogen peroxide to obtain a compound II; the content of the meta-chloroperoxybenzoic acid in the first solution is more than 1 times of the amount of substance of the compound I; performing a reduction reaction on the compound II under the action of hydrogen and a catalyst to obtain a compound III; performing a hydrolysis reaction on the compound III in a dilute acid solution, and then performing a hydroxyl elimination reaction on the compound III in a second solution to obtain the dydrogesterone; the structural formulae of the compound I, the compound II, the compound III and the dydrogesterone are as follows:; and. The preparation method has less by-products and a higher reaction yield.

The invention relates to the field of fuel cells, in particular to a non-platinum electrocatalytic hydrogen evolution catalyst and a preparation method and application thereof.The preparation method comprises the steps that S1, an ammonium persulfate solution is added into an aniline solution, standing is conducted for 24-36 hours at the room temperature, and first powder is obtained after centrifugation, filtration, washing and drying are conducted; s2, adding the first powder and dichloromethane into a container, preserving heat at the temperature of 0 DEG C, stirring for 15-30 minutes, dropwise adding m-chloroperoxybenzoic acid into the container, continuously preserving heat at the temperature of 0 DEG C, and stirring for 1-3 hours to obtain first liquid; s3, stirring the first liquid at room temperature for 18-48 hours, and filtering to obtain second powder; s4, under the protective atmosphere, the second powder is subjected to heat preservation for 2-6 hours at the temperature of 600-1100 DEG C, and third powder is obtained; and S5, carrying out ball milling on the third powder and dichlorodiaminoacetic acid for 2-4 hours to obtain fourth powder, and carrying out heat preservation on the fourth powder at 800-1000 DEG C in a protective atmosphere for 1-3 hours to obtain the non-platinum electro-catalytic hydrogen evolution catalyst which can reduce the cost of the fuel cell catalyst.

The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of substituted phenylene aromatic diester and application of the substituted phenylene aromatic diester in catalyst preparation. The preparation method comprises the following steps: firstly, enabling 2-hydroxy-3-methyl benzaldehyde to react with m-chloroperoxybenzoic acid and sodium ethoxide to generate 3-methyl catechol; then, triisobutyl aluminum is used as a catalyst, 3-methylcatechol and isobutene are subjected to a reaction, and 5-tert-butyl-3-methylcatechol is generated; finally, the 5-tert-butyl-3-methyl catechol reacts with triethylamine and benzoyl chloride, and the 5-tert-butyl-3-methyl catechol is obtained. According to the novel preparation method of the substituted phenylene aromatic diester, by selecting the specific alkaline reagent and the catalyst, the dependence of a traditional reduction method on a metal reagent is avoided, the yield and the purity of the substituted phenylene aromatic diester are greatly improved, the reaction condition is mild, the cost is low, and the method is suitable for large-scale preparation.

The present application relates to a kind of recycling method of avibactam intermediate production waste liquid, belong to pharmaceutical chemical technology field;The present application will be in the 5-benzyloxyamine piperidin-2S-formic acid ethyl ester oxalate in avibactam intermediate production waste liquid by desalination into free state, under the condition of ethyl acetate as solvent, using the dilute solution of m-chloroperbenzoic acid drop, homogeneous reaction in organic solvent, effectively improve the utilization of raw material, with the advantage of less by-product, and have higher recovery rate than prior art, in addition, the present application also prepares a kind of activated carbon loaded sodium triacetoxyborohydride, can play the role of catalytic sodium triacetoxyborohydride reduction amination reaction, improve the utilization of sodium triacetoxyborohydride, and prevent sodium triacetoxyborohydride from contacting with water.

The invention discloses a synthesis method of limidoterol, and belongs to the technical field of medicine synthesis. The method comprises the following steps: coupling cyclobutanone oxime and a caffeic acid derivative under the catalysis of ferrous acetylacetonate, a chlorobenzene solvent and the protection of nitrogen to obtain a decarboxylated cyanogen alkylation intermediate; oxidizing the intermediate with m-chloroperoxybenzoic acid in dichloromethane in the presence of sodium carbonate to obtain a vicinal diol monoester intermediate; catalyzing by cobalt chloride in methanol, reducing by sodium borohydride, and protecting by Boc2O to obtain a cyclized precursor; cyclizing the precursor in tetrahydrofuran by using sodium hydride to obtain a cyclized intermediate; and performing deprotection to obtain the limiterol. According to the method, dangerous reagents and processes are not used, the safety is high, and no heavy metal residues exist; the cost is low, precious metals are not needed, the post-treatment operation is simple and convenient, a complex purification process is not needed, and the total yield reaches 21%; process conditions are mild, normal pressure and conventional heating modes are adopted, and industrial production is easy to realize.

The invention belongs to the field of organic synthesis, and discloses a synthesis method of a 2-indanone compound. According to the method, an indene compound is used as a raw material, m-chloroperoxybenzoic acid is used as an oxidizing agent, and oxidation migration occurs in a dichloromethane solution at the temperature of 30-50 DEG C to obtain the 2-indanone compound. According to the method, transition metal and lewis acid do not need to be additionally added, and the method has the high green and environment-friendly advantages; the method also has the advantages of mild reaction conditions, low price of the used oxidant, simple post-treatment operation and the like; a novel synthesis method is developed for the 2-indanone compound, and the 2-indanone compound has good research value and practical application prospect.

The application belongs to the technical field of organic synthesis, and particularly relates to a preparation method of substituted phenylene aromatic diester and application thereof in preparation of a catalyst. The preparation method comprises the following steps: first, 2-hydroxy-3-methylbenzaldehyde is reacted with meta-chloro peroxybenzoic acid and sodium ethoxide to generate 3-methyl catechol; then, 3-methyl catechol is reacted with isobutene by taking triisobutyl aluminum as a catalyst to generate 5-tert-butyl-3-methyl catechol; finally, 5-tert-butyl-3-methyl catechol is reacted with triethylamine and benzoyl chloride, and the substituted phenylene aromatic diester is obtained. The application provides a novel preparation method of the substituted phenylene aromatic diester, the dependence on metal reagents in a traditional reduction method is avoided by selecting specific alkaline reagents and catalysts, the yield and purity of the substituted phenylene aromatic diester are greatly improved, the reaction condition is mild, the cost is low, and the method is suitable for large-scale preparation.

The invention discloses a high-temperature-resistant hot-melt pressure-sensitive adhesive and a preparation method thereof, and relates to the technical field of adhesives. The high-temperature-resistant hot-melt pressure-sensitive adhesive prepared by the invention comprises a thermoplastic elastomer, branched polyolefin, modified tackifying resin and an auxiliary agent, the branched polyolefin is prepared by reaction of 1, 2, 4-cyclohexane trimethyl anhydride, a sulfydryl block polymer and an epoxy polyolefin elastomer, and the sulfydryl block polymer is prepared by reaction of tert-butyl acrylate, 4-vinyl benzyl chloride and potassium thioacetate and then thioacetate removal reaction. The epoxy polyolefin elastomer is prepared from a polyolefin elastomer and m-chloroperoxybenzoic acid through a reaction, the modified tackifying resin is prepared from p-tert-octylphenol formaldehyde resin and a multi-benzene-ring compound through a reaction, the multi-benzene-ring compound is prepared from pyromellitic dianhydride, diethanol amine and epoxy polyisoprene through a reaction, and the heat resistance and cohesiveness of the hot-melt pressure-sensitive adhesive are improved. The invention discloses a manufacturing method of a high-emissivity coating suitable for the surface of a refractory material.

The invention discloses a preparation method of a tigecycline USP impurity G. The tigecycline USP impurity G is obtained by taking tigecycline as a raw material, adding an oxidizing agent metachloroperbenzoic acid, and carrying out oxidation rearrangement reaction, separation and purification. The invention discloses a method for preparing a tigecycline USP impurity G, and aims to provide a method for preparing the tigecycline USP impurity G. The purity of a target product obtained through the method is 95% or above, the target product can be directly used as a tigecycline impurity detection reference substance, specific economic benefits are generated, and the method has a good application prospect. Belongs to the technical field of medicine.

The invention relates to the technical field of crude oil component analysis, in particular to a method for analyzing olefin compounds based on epoxy three-membered ring reaction, which comprises the following steps: mixing an olefin-containing substance to be detected with a reaction reagent for derivatization reaction, the reaction reagent being metachloroperbenzoic acid; and carrying out mass spectrometry on the product of the derivatization reaction to obtain a mass spectrum, and deducing the number of double bonds of the olefin compound in the to-be-detected substance through the mass spectrum. The method can be used for high-sensitivity detection of olefin in complex matrixes such as petroleum product oil and the like, olefin molecules containing six double bonds can be identified, and identification of fine structures of the double bonds can be carried out on various types of olefin compounds. In the detection process, a catalyst and photocatalysis do not need to be additionally added, a good result can be generated only through one oxidizing reagent, a good detection effect can be achieved only through 5 minutes of reaction, detection is rapid and efficient, operation is easy, and selectivity is high.

The invention provides a method for synthesizing m-chloroperoxybenzoic acid by a multi-stage series circulating tube type continuous reactor, and belongs to the technical field of chemical production. According to the method, m-chlorobenzoyl chloride, hydrogen peroxide, inorganic alkali and inorganic acid are used as raw materials, sulfate is used as a stabilizer, and the raw materials are simultaneously and continuously fed into a multi-stage series circulating tube type continuous reactor for a synthetic reaction under the condition of a solvent. The yield of the m-chloroperoxybenzoic acid can reach 95% or above, and compared with an existing process, the yield is increased by 17-20%; according to the invention, an intermittent / semi-intermittent kettle type process is improved into a continuous circulating pipe type process, so that the automatic and continuous production level is improved.

The invention provides a preparation method of 4-chloro-6, 7-dihydro-5H-cyclopenta [B] pyridine-7-alcohol, and relates to the technical field of organic synthesis. A compound 1 and first m-chloroperoxybenzoic acid are subjected to a first oxidation reaction to obtain a compound 2 crude product, the compound 2 crude product and acid anhydride are directly subjected to a Boekelhede reaction to obtain a compound 3, the water solubility of the compound 3 is poor, the compound 3 is easily separated from a water-soluble byproduct m-chlorobenzoic acid, and a large amount of loss of the compound 3 in the subsequent separation process cannot be caused; the yield of the compound 3 is improved; and carrying out a second oxidation reaction on the compound 3 and second m-chloroperoxybenzoic acid, carrying out a chlorination reaction on the obtained compound 4 and phosphorus oxychloride, and carrying out a hydrolysis reaction on the obtained compound 5 to obtain the 4-chloro-6, 7-dihydro-5H-cyclopenta [B] pyridine-7-ol. According to the preparation method provided by the invention, the total yield of the 4-chloro-6, 7-dihydro-5H-cyclopenta [B] pyridine-7-alcohol is high.

The invention discloses a high-efficiency synthesis method of a 2-aryl-1-indanone compound, which comprises the following steps of: heating an indene compound serving as a raw material and m-chloroperoxybenzoic acid serving as an oxidant in an organic solvent to react, removing the solvent after the reaction is finished, and separating to obtain the 2-aryl-1-indanone compound. The reaction formula of the synthesis method is as follows: in the formula, R1 is selected from hydrogen atom, methyl, chlorine, trifluoromethyl or fluorine; r2 is selected from methyl, ethyl or n-butyl; and R3 is methyl, fluorine, chlorine or tertiary butyl. The oxidant used in the method is low in price, so that the reaction cost is reduced, and the post-treatment steps of the reaction are simplified. The synthesis reaction does not need inert gas protection atmosphere, the operation is simple and convenient, the reaction condition is mild, and the yield is up to 90%.

The invention discloses a preparation method of a tetra-functional alicyclic epoxy compound, which comprises the following steps: mixing pentaerythritol, 3-cyclohexene-1-formic acid, a catalyst and an organic solvent to obtain a solid-liquid mixture, dropwise adding a condensing agent into the solid-liquid mixture, dissolving the condensing agent into the organic solvent to obtain a first mixed solution, stirring until solids in the solid-liquid mixture are dissolved, reacting for 16-24 hours, filtering, washing, and drying to obtain the tetra-functional alicyclic epoxy compound. Washing and drying a reaction system after the reaction to obtain an organic phase, then carrying out reduced pressure distillation on the organic phase, and crystallizing residues of the organic phase obtained after the reduced pressure distillation to obtain pentaerythritol tetracyclohexene formate; the preparation method comprises the following steps: dissolving pentaerythritol tetracyclohexene formate into an organic solvent to obtain a second mixed solution, dissolving metachloroperbenzoic acid into the organic solvent to obtain a third mixed solution, dropwise adding the third mixed solution into the second mixed solution under the condition of ice bath, stirring, reacting for 16-24 hours, filtering, purifying the filtrate to obtain an organic phase, and drying to obtain the product. The method is mild in reaction condition, and the yield of the four-functional alicyclic epoxy compound is improved.

The present invention discloses a method for synthesizing N-trifluoromethylsulfonamide compounds. The method uses aromatic isothiocyanates as starting materials and utilizes a series of reagents, including silver fluoride, triethylsilane, p-toluene thionyl chloride, m-chloroperbenzoic acid, and potassium fluoride, to synthesize N-trifluoromethylsulfonamide compounds through a multi-step reaction. The present invention introduces a trifluoromethyl group into the sulfonamide structure, while maintaining mild reaction conditions and utilizing a wide range of raw material sources.

The invention relates to the field of fuel cells, in particular to a ZIF-derived non-noble metal electrocatalyst and a preparation method thereof.The preparation method comprises the steps that H3BTT. 2HCl and trichloromethane are added into a container, m-chloroperoxybenzoic acid is dropwise added, and a first solution is obtained; sealing the container, preserving heat, stirring the first liquid, naturally cooling, adding methylbenzene, stirring the first liquid, and irradiating ultraviolet rays for several hours to obtain a second liquid; opening the container, adding pyridine and ammonium carbonate, and stirring to obtain a third solution; carrying out heat preservation on the third liquid, and sequentially introducing mixed gas of ozone and oxygen for bubbling, introducing pure oxygen for bubbling and introducing nitrogen for bubbling to obtain fourth liquid; carrying out heat preservation and stirring on the fourth liquid, filtering and drying to obtain first powder; adding the first powder and anhydrous ferrous chloride into a mixed solution of dimethylformamide and dimethyl sulfoxide, carrying out heat preservation stirring, filtering and drying to obtain second powder; the second powder is subjected to heat preservation, and the ZIF-derived non-noble metal electrocatalyst is obtained and can reduce the cost of a polymer electrolyte membrane fuel cell.

The invention relates to the fields of coordination chemistry and metal organic chemistry, and discloses a metal-only center chiral osmium carbon dragon complex as well as a preparation method and application thereof. According to the synthesis method, a chiral polyalkyne carbon chain (a carbon dragon ligand precursor containing a propargyl alcohol structure unit) with pure enantiomers is reacted with a metal osmium source OsCl2 (PAr3) 3, and the chirality of a carbon center on the polyalkyne carbon chain is transferred to the chirality of a metal center of the carbon dragon complex through a chiral transfer strategy, so that the one-pot preparation of the metal-center-only chiral osmium carbon dragon complex is realized. The synthesis method has the characteristics of simplicity and convenience in operation, easiness in separation, mild reaction conditions, easiness in obtaining of raw materials, good universality of reactants and the like. And meanwhile, the obtained metal-center-only chiral osmium carbon long complex can react with various reagents such as m-chloroperoxybenzoic acid / sulfur powder / tin powder / cuprous chloride / silver tetrafluoroborate, phenanthroline / triphenylphosphine gold chloride / acetonitrile / pyridine / imidazole and the like, so that further derivatization is realized, and a series of brand new metal-center-only chiral osmium carbon long complexes are obtained. The metal-only center chiral osmium-penta-oxa three-membered ring complex provided by the invention can be used for efficiently catalyzing an asymmetric Michael addition reaction of indole and an alpha-hydroxyl-alpha ', beta'-unsaturated ketone compound.

The invention belongs to the technical field of medicines, and particularly provides a novel synthesis method of a dotenorad crude product, which comprises the following steps: by taking 2-aminobenzenethiol as a starting material, carrying out cyclization reaction, primary oxidation reaction, acylation reaction and secondary oxidation reaction to obtain the dotenorad crude product; the characteristic of relatively weak oxidability of hydrogen peroxide is mainly utilized; thioether (1) is difficult to directly and completely oxidize into sulfuryl (2 ') in a high-yield form, instead, m-chloroperoxybenzoic acid with relatively high price is used for completing thorough oxidation, and the oxidation of thioether is controlled by controlling the equivalent weight of hydrogen peroxide, a composite catalyst and a catalytic promoter, so that the yield of sulfuryl (2') is greatly improved. In the synthesis process, most of oxidation products stay in a sulfoxide structure (2) and are difficult to be completely converted into a sulfuryl structure, and the oxidation reaction is performed again, so that the use amount of m-chloroperoxybenzoic acid can be relatively reduced, and the synthesis cost of a dotenorad crude product is reduced.

The invention relates to a recycling method of avibactam intermediate production waste liquid, and belongs to the technical field of pharmaceutical chemicals. According to the method, 5-benzyloxyamino piperidine-2S-ethyl formate oxalate in the avibactam intermediate production waste liquid is desalted to be in a free state, under the condition that ethyl acetate serves as a solvent, a diluted solution of m-chloroperoxybenzoic acid is dropwise added, homogeneous reaction is carried out in the organic solvent, the utilization rate of raw materials is effectively increased, and the yield is increased. Compared with the prior art, the method has the advantages that by-products are few, the recovery rate is higher than that in the prior art, in addition, activated carbon loaded sodium triacetoxyborohydride is further prepared, the effect of catalyzing the reductive amination reaction of sodium triacetoxyborohydride can be achieved, the utilization rate of sodium triacetoxyborohydride is increased, and the yield of sodium triacetoxyborohydride is increased. The sodium triacetoxyborohydride is prevented from being in contact with water.

The invention relates to the technical field of preparation of enantiomer pure amine, and particularly discloses a JM01 purification preparation method which comprises the following steps: carrying out reaction on cyclohex-3-ene-1 (R)-formic acid, methylbenzene, triethylamine, diphenyl azide phosphate DPPA, tert-butyl alcohol and cuprous chloride CuCl to prepare (R)-4-(BOC-amino) cyclohexene N-BOC; reacting the N-BOC with m-chloroperoxybenzoic acid (mCPBA) and dichloromethane, so as to obtain tert-butyl ((1R, 3R, 6S)-7-oxabicyclo [4.1. 0] heptane-3-yl) carbamate O-BOC; obtaining {(1R, 2R, 4R)-4-[(t-butyloxycarbon)-amino]-2-hydroxycyclohexyl} phenyl thioester JM01 from the O-BOC, toluene thiobenzoate and tetrabutylammonium chloride monohydrate, and obtaining {(1R, 2R, 4R)-4-[(t-butyloxycarbon)-amino]-2-hydroxycyclohexyl} phenyl thioester JM01; according to the present invention, the column chromatography is adopted to replace the technology, and the efficient purification of the difficult-to-crystallize compound is successfully achieved by using the developed gradient cooling crystallization system and combining the n-heptane-toluene composite solvent system according to the characteristic that the intermediate is easily dissolved in the organic solvent; compared with traditional column chromatography, the process time is greatly shortened, and the solvent consumption is reduced.

The invention relates to the technical field of preparation of photoacid generators, in particular to a preparation method and application of (4-fluorophenyl) diphenyl sulfonium trifluoromethanesulfonic acid. The preparation method comprises the following steps: mixing p-iodofluorobenzene, fluorobenzene and m-chloroperoxybenzoic acid to obtain a mixed raw material; carrying out substitution reaction on trifluoromethanesulfonic acid and the mixed raw material to obtain an intermediate product; wherein the intermediate product has a structural formula shown as a formula 1, and in the formula 1, TfO is a trifluoromethanesulfonic acid anion; under the condition that copper acetylacetonate is used as a catalyst, diphenyl sulfide and the intermediate product are subjected to a catalytic reaction, and the (4-fluorophenyl) diphenyl sulfonium trifluoromethanesulfonic acid is obtained. The preparation method can effectively and synchronously improve the yield of the (4-fluorophenyl) diphenylsulfonium trifluoromethanesulfonic acid to 70% or above and the purity of the (4-fluorophenyl) diphenylsulfonium trifluoromethanesulfonic acid to 99.0% or above based on coordination of reaction step-by-step refinement, electronic effect, structural stability and catalytic action.

The present invention relates to a preparation method of montelukast sodium intermediate, belonging to the field of pharmaceutical chemistry. In the present invention, crotonic acid is used as the starting material, and ethyl 3-butenoate is generated through esterification rearrangement reaction. The double bond of ethyl 3-butenoate undergoes epoxidation reaction with m-chloroperoxybenzoic acid to obtain an epoxy compound. The epoxy compound reacts with thiourea to obtain a cyclic sulfur compound. The cyclic sulfur compound undergoes ring opening with a cuprous salt reagent and cyclopropylmagnesium bromide, and finally, it is further hydrolyzed under alkaline conditions to obtain 1-mercaptomethylcyclopropylacetic acid. This method has cheap and easily available starting materials, reducing the material cost; in the reaction process, the use of highly toxic cyanide reagents or extremely explosive diazomethane is avoided, improving the production safety, and the technological process is simple and easy to implement; the number of reaction steps is reduced, the production cost can be greatly reduced, which is beneficial to industrial production.